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J Food Sci Technol (July–August 2011) 48(4):460–465

DOI 10.1007/s13197-010-0126-x

ORIGINAL ARTICLE

Physicochemical, morphological and pasting properties


of acid treated starches from different botanical sources
Manmeet Kaur & D. P. S. Oberoi & D. S. Sogi &
Balmeet Singh Gill

Revised: 18 January 2010 / Accepted: 23 January 2010 / Published online: 29 October 2010
# Association of Food Scientists & Technologists (India) 2010

Abstract Effect of acid modification on physico-chemical, esterification and cross-linking. Various methods such as
morphological and pasting properties of banana, sweet acid, phosphate and H2O2 treatments can be employed to
potato, lotus stem and wheat starches were studied. Results modify starch (Akubor 2007). The objective of starch
revealed that swelling power, solubility and water binding modification is to alter the physico-chemical characteristics
capacity of all starches decreased by acid modification. By of native starch to improve functional characteristics.
acid modification starch granules from different varieties Modification is important for the continued and increased
tended to appear fused and less smooth than the native use of starch to provide thickening, gelling, binding,
starch granules. The pasting properties of native starches of adhesiveness and film forming characteristics.
all different varieties have significantly decreased following Swelling power indicates the water holding capacity of
acid modification. Acid modified starches showed higher starch, which has generally been used to demonstrate
syneresis as compared to native starches. differences between various types of starches (Crosbie
1991). Swelling volume is the ratio of the sedimented gel to
Keywords Starch . Acid modification . Pasting properties . the dry weight of starch. Solubility is the percent amount of
Morphological properties starch leached out into the supernatant in the swelling
volume determination (Singh et al. 2005). The water
binding capacity in commercial starches is important to
Introduction the quality and texture of some food products because it
stabilize them against effects such as syneresis, which
Starch is the major reserve polysaccharide in plants and is sometimes occurs during retorting of freezing (Baker et al.
in the form of granules that exist naturally within the plant 1994). Scanning electron microscopy has been used to
cells. Starch can be used as thickener, an adhesive, binder, relate granules morphology to starch genotype (Fannon et
encapsulating agent, film former, gelling agent, water al. 1992). Rapid visco-analyser (RVA) has been extensively
binder, texturizer and fat-sparing agent and with numerous used for measuring starch paste viscosity. Pasting properties
other applications both in the food and non-food areas helps in comparison between cooking behaviour of differ-
(Mauro 1996). Starch granules are composed of a mixture ent starches with the aid of RVA thermal viscous graph. The
of two polymers, an essentially linear polysaccharide called present study was undertaken to investigate the effect of
amylose and a highly branched polysaccharide called acid modification on physicochemical, morphological and
amylopectin (Bemiller and Whistler 1996). Starch can be pasting properties of starches extracted from different plant
modified by acid hydrolysis, oxidation, etherification, sources.

M. Kaur : D. P. S. Oberoi : D. S. Sogi : B. S. Gill (*) Material and methods


Department of Food Science and Technology, Guru Nanak Dev
University,
Amritsar 143005, India Freshly harvested sweet potato (Ipomoea botatas), green
e-mail: balmeet_singh@yahoo.co.in un-ripened bananas (Musa acuminata) and lotus stem
J Food Sci Technol (July–August 2011) 48(4):460–465 461

(Nelumbo nucifera) was procured from the local market, Acid modification Dry starch (100 g) was taken in a beaker
Amritsar, India. ‘PBW-373’ wheat (Triticum aestivum) and 150 ml of 6% (w/v) HCl at 40 °C were added in
variety was procured from PAU, Ludhiana, India. batches over 48 h with occasional stirring. Acid addition
was done carefully to accomplish a uniform dispersion of
Isolation of starch Banana fruits were peeled, cut into starch throughout the acid. After each hydrolysis, the
6 mm slices, each slice was cut into four pieces and dipped suspension was neutralized with 2% (w/v) NaOH solution
immediately in sodium bisulphate solution (0.25 g/l) in 2:1 and washed three times with distilled water. The water was
(v/w) proportion. Fruit pieces were macerated and blended then removed by centrifugation at 3000 rpm for 10 min and
(Sujata, New Delhi, India) at low speed 100 rpm for 5 min. decantation. The wet acid-modified starch was dried in hot-
The resultant slurry was sieved through 100 mesh until the air-oven at temperature not exceeding 40 °C. The dried
waste solution was clean. Starch suspension was left powder was ground and sieved through 100-mesh sieve to
overnight at refrigerated temperature (4 °C) and washed obtain acid-modified starch powder.
with tap water, centrifuged (Eltek, Mumbai, India) at
3000 rpm for 15 min. The white sediment was dried at
40 °C in a convection oven (Universal, New Delhi, India)
for 24 h, ground in a pestle and mortar, passed through a Physico-chemical properties
100 mesh screen and stored in sealed glass jars at room
temperature (25–30 °C) (Waliszewski et al. 2003). Swelling power and solubility A solution of starch slurry
The lotus stems were washed, peeled, cut into small pieces (1%) was made and heated in water-bath (Gupta Pvt Ltd,
and ground in a blender to form a paste. The resultant slurry Ambala Cantt, India) maintained at 90 °C for 30 min with
was sieved through 100 mesh linen cloth into a beaker. Starch constant stirring and cooled. The suspension was centri-
suspension was left overnight and extracted by washing with fuged at 3200 rpm for 10 min and the supernatant collected
distilled water by four times. The resultant slurry was in a pre-weighed aluminium dish, which was evaporated at
centrifuged at 3200 rpm for 10 min. The isolated starch was 110 °C for 24 h. The dried aluminium dishes were weighed
dried in an air oven at 40 °C for 24 h. for calculation of solubility. The weight of wet sediment in
Sweet potatoes were washed thoroughly, immersed in centrifuge tube was noted to determine the swelling power
ice cold water for 1 h, peeled, sliced and steeped in 0.1% (Leach et al. 1959).
(w/v) potassium metabisulphite to control enzymatic
browning. It was then ground in a blender to form a paste. Water binding capacity A suspension of 2.5 g native and
The recovery of the paste was done in 4% (w/v) NaCl treated sample in 20 ml of distilled water was agitated
solution. The solution was sieved and allowed to settle for 30 min in a shaker (Narang Scientific Works, New
overnight. The starch was extracted by washing with Delhi, India). The suspension was poured into pre-
distilled water four times. The resultant slurry was weighed centrifuge tube. Then 10 ml of distilled water
centrifuged at 3200 rpm for 10 min. The isolated starch used for rinsing starch from beaker, which was also
was dried in an air oven at 40 °C for 24 h (Collado and added to centrifuge tube and centrifuged at 3000 rpm for
Corke 1997). 10 min. Supernatant was decanted and wet starch was
Stiff dough was prepared by mixing 100 g of wheat flour weighed to determine water binding capacity (Anderson
with 45–55 ml of distilled water, left for 1 h at room et al. 1969).
temperature (30 °C), covered with moistened cheese cloth.
It was washed under water gently to separate starch from Scanning electron microscopy (SEM) Scanning electron
gluten, over the mouth of beaker over a nylon mesh micrographs were obtained at 800x with a SEM (Joel
(240 μm). The water-starch suspension was allowed to JSM-6100, Jeol Ltd., Tokyo, Japan). Starch samples were
settle for 5–7 h at 7 °C. The supernatant was decanted and suspended in ethanol to obtain a 1% suspension. One drop
starch slurry was recovered. The slurry was centrifuged at of the starch-ethanol solution was applied on an aluminium
3000 rpm for 10 min. The upper pigmented fraction was stub using double-sided tape and the starch was coated with
removed carefully by scraping with metal spatula. The gold-palladium (60:40). An accelerating potential of 10 KV
sediment was re-suspended in distilled water and centri- was used during micrography.
fuged again, scrapped-off in same way after 3–4 washings Pasting properties of native and acid modified starches
to obtain purified starch. The resultant starch sediments were studied using RVA (RVA-4 D, Warriewood, Australia).
were dried at 40 °C in hot-air-oven overnight and clumps Three g sample along with 25 g distilled water were weighed
were broken manually to prevent formation of hard masses. into aluminium canister. Paddle was placed into canister and
The clumps were finally ground and passed through 72 vigorously jocked 10 times up and down to break any lumps
mesh sieve (Wolf 1964). on water surface. The sample was equilibrated at 50 °C for
462 J Food Sci Technol (July–August 2011) 48(4):460–465

1 min, heated to 95 °C in 4.42 min, held at 95 °C for 3.1 min of reagents in granules. During acid modification hydroxo-
before cooling to 50 °C and holding at 50 °C for 2 min. The nium ion (H3O+) attacks glycosidic O2 atom and hydrolyse
mixture was stirred at 960 rpm for 10 s and then at 160 rpm for glycosidic linkage, therefore acid preferentially attacks at
remainder of the test. amorphous regions. This causes increase in solubility index
Starch suspension (2%, w/w) was heated at 85 °C for of acid modified starches.
30 min in a temperature controlled water bath (Gupta Pvt
Ltd, India), followed by rapid cooling in an ice water bath Water binding capacity The acid modification reduced
to the room temperature. The starch sample was stored for water binding capacity of starch (Table 1). Acid thinning
1, 2, 3, 4 and 5 days at 4 °C. Syneresis was measured impaired both hydrophilic and hydrophobic capacities of
(triplicates) as amount (%) of water released after centrifu- native starch. The acid thinning reduces water absorption
gation at 3000 rpm for 15 min. capacity because of increase in crystalline region and
decrease in amorphous region in starch granules that
Statistical analysis The mean and standard deviation of reduced the number of available binding sites thus lowering
morphological and pasting properties parameters were the water binding capacity (Lawal 2004).
calculated. One way ANOVA and least significant differ-
ence were employed to check the significant effect (p< Pasting properties The pasting temperature of acidified
0.05) of acid modification on the morphological and starches was higher than native starches (Table 2). The acid
pasting properties of starches extracted from different hydrolysis removed amorphous regions of starch granules
botanical sources (Cochran and Cox 1957). leading to lowering of viscosity. The final viscosity of acid
thinned modified starches was more than peak and hot paste
viscosity. Acid modified starches show higher final viscosity
supporting the fact that amylose terminated the short term gel
Results and discussion structure development (Wang and Wang 2001). Kaur et al.
(2007) studied on the effect of aqueous HCl on properties of
Swelling power and solubility index The swelling power of wheat starch and found that the pasting temperature, peak
acid modified starches was lower in all cases as compared viscosity, hot paste viscosity and cold paste viscosity showed
to native starches (Table 1). Kaur et al. (2007) studied the a decline with acid modification.
effect of aqueous HCl on properties of wheat starch and
found that swelling power decreased from 15.4 to 5.0 g/g Morphological properties The starches have been reported
with increase in modification time. The reduction in to differ in granules size, shape, presence of phosphate
swelling power of acid modified starches was reported esters, amylose to amylopectin ratio that in turn is
due to increase in high proportion of soluble dextrins of responsible for rheological, thermal and other functional
both small and medium chain lengths in starch granules properties (Wisenborn et al. 1994). The granules size and
(John et al. 2002). geometry differed significantly among various starches.
Solubility index of native starches was lower compared The granules from different starches showed spherical,
to acid modified starches (Table 1). Fannon et al. (1992) oval, cylindrical and oblong shapes but oval, cylindrical
reported that channels present in starch granules may also and irregular shapes were predominant. The native banana
be responsible for aiding permeation and increase the starch granules showed size in the range of 10–27 μm with
potential surface area available for reaction and penetration higher proportion of medium size granules (Fig. 1). After

Table 1 Swelling power, solubility and water binding capacity of native and acid modified starches

Starch from Swelling power, g/g Solubility,% Water Binding capacity,%

Native Acid modified Native Acid modified Native Acid modified

Banana 16.0c ±0.41 0.48c ±0.03 8.1b ±0.35 51.1d ±0.97 107.7a ±3.04 71.7a ±1.01
Lotus Stem 31.0a ±1.26 0.80b ±0.7 2.4c ±0.42 62.4b ±1.13 100.5b ±3.03 61.6b ±1.17
Sweet Potato 21.5b ±0.15 0.72b ±0.14 7.8b ±0.76 67.7a ±0.83 78.1c ±2.66 57.0c ±0.70
Wheat 9.8d ±0.60 1.05a ±0.07 12.9a ±1.03 55.7c ±1.06 66.8d ±2.05 46.4d ±1.20

* Means with different superscripts are significantly different (p≤0.05) along the rows (n=3)
J Food Sci Technol (July–August 2011) 48(4):460–465 463

Table 2 Pasting properties of native and acid modified starches

Starch PT, °C PV, cp HPV, cp Native CPV, cp BD, cp SB, cp

Banana 75.1a ±0.29 4577b ±2.9 3532.7d ±18.5 4364d ±59 1045b ±33.9 832b ±41.1
Lotus stem 74.9a ±0.89 8314d ±330 2673b ±35.1 3471b ±60.8 564a ±35.9 798b ±90.5
Sweet potato 74.2a ±0.02 5964.3c ±43.5 2960c ±23.2 3587c ±93.1 3005c ±23.7 627a ±27.8
Wheat 81.6b ±4.33 2810.0a ±7.0 2243a ±48.3 3370a ±32.5 567a ±51.8 1127c ±27.9
Acid modified
Banana 78.2a ±0.01 285.7a ±6.66 210.7a ±7.02 316.3a ±4.04 75a ±1 105.7a ±3.21
Lotus stem 77.4a ±0.77 516.0d ±67.6 318.0d ±47.8 624.0c ±2.04 198c ±20.2 306c ±156.8
Sweet potato 76.4a ±0.46 466.7c ±33.2 241.3c ±14.15 453.0b ±11.53 225.3d ±24 205b ±9
Wheat 94.9b ±0.5 329.7b ±44.6 235.0b ±48.6 635.7c ±48 94.7b ±4.04 400.7d ±4.16

PT Pasting temperature; PV Peak viscosity; HPV Hot paste viscosity (Minimum viscosity at 95 °C); CPV Cold paste viscosity (Final viscosity at
50 °C); BD Breakdown viscosity; SB Setback viscosity; cP Centipoise
* Means with different superscripts are significantly different (p≤0.05) along the rows (n=3)

acid modification the granule size increased and reported a the modified wheat granules had sizes in the range of 12–
range of 15–34 μm. The native lotus starch granule showed 21 μm. Wheat granules seem to be affected more by acid
uniform size, oblong structure having average granule size hydrolysis compared to other acid modified granules.
in the range of 14–31 μm which increased to 25–37 μm
after acid modification. The native sweet potato show Syneresis The syneresis of the native and acid modified
granule size range of 8–20 μm which after acid modification banana, lotus stem, sweet potato and wheat after 1, 2, 3, 4
was reported to vary from 8 to 18 μm (Fig. 2). There was and 5 days (Table 3) was analyzed. The acid modified
slight reduction in size in case of sweet potato granules after sample showed higher syneresis compared to native
acid modification. The native wheat starch granules had sizes starches. The initial gel firmness during gelation is
in the range of 9–28 μm with fairly uniform proportion of attributed to the formation of amylose matrix gel and slow
large, medium and small granules. After acid modification, increase in gel firmness due to amylopectin crystallization.

Fig. 1 Scanning electron


microscopy photographs of
banana starch. (A-Native,
B-Acid modified) and Lotus
stem starch (C-Native, D-Acid
modified)
464 J Food Sci Technol (July–August 2011) 48(4):460–465

Fig. 2 Scanning electron


microscopy photographs of
sweet potato starch. (E-Native,
F-Acid modified) and wheat
starch (G-Native, H-Acid
modified)

The amount of water excluded from the starch gel system phological properties revealed hydrolysis of starch
stored at low temperature is due to increase in intermolec- granules due to attack of acid on amorphous regions,
ular and intra molecular hydrogen bonding due to interac- which come in contact with the acid leading to fusion of
tion between amylose- amylose, amylose- amylopectin and granules. After modification, starch granules tended to
amylopectin- amylopectin chains. appear fused and less smooth than the native starch
granules. The acid modified starches reported slightly
higher pasting temperature compared to their native
counterparts. The acid modification reduced thickening
Conclusion ability of starches that is based on swollen capacity of
undamaged granules as revealed by pasting properties.
Swelling power, solubility and water binding capacity of The syneresis increased with acid modification of
starches decreased following acid modification. The mor- starches.

Table 3 Effect of acid


modification on the syneresis Storage (4 °C) period, days
(%) of native and modified
starches during storage Starch from 1 2 3 4 5

Native
Banana 15.7ap ±0.71 18.8aq ±0.37 20.2ar ±0.34 21.2as ±0.78 21.3bs ±0.35
Lotus stem 11.4 bp ±0.39 13.8bq ±0.28 15.7br ±0.28 21.9as ±0.50 23.8as ±0.22
Sweet potato 9.8cp ±0.40 13.8bq ±0.24 15.8br ±0.32 18.7bs ±0.65 18.8cs ±0.33
Wheat 7.2dp ±0.25 8.4cq ±0.23 10.8cr ±0.37 12.7cs ±0.42 13.9dt ±0.21
Acid modified
Banana 29.7ap ±0.40 31.9ap ±0.50 32.8ap ±0.30 35.8aq ±0.34 41.6br ±0.60
* Means with different
superscripts are significantly Lotus stem 28.5 bp ±0.24 30.0 bp ±0.29 32.8aq ±0.28 35.8ar ±0.39 43.6as ±0.20
different (p≤0.05) along the Sweet potato 18.6dp ±0.32 19.6dp ±0.21 23.7cq ±0.15 26.9cr ±0.32 32.3ds ±0.34
rows (a,b,c...) and columns (p, Wheat 22.8cp ±0.20 23.7cp ±0.30 25.8bq ±0.37 28.7br ±0.18 33.8cs ±0.85
q, r...) (n=3)
J Food Sci Technol (July–August 2011) 48(4):460–465 465

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